WO2012161168A1 - Procédé de récupération de matériaux de valeur dans l'électrode positive d'un accumulateur lithium-ion - Google Patents

Procédé de récupération de matériaux de valeur dans l'électrode positive d'un accumulateur lithium-ion Download PDF

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Publication number
WO2012161168A1
WO2012161168A1 PCT/JP2012/062981 JP2012062981W WO2012161168A1 WO 2012161168 A1 WO2012161168 A1 WO 2012161168A1 JP 2012062981 W JP2012062981 W JP 2012062981W WO 2012161168 A1 WO2012161168 A1 WO 2012161168A1
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WIPO (PCT)
Prior art keywords
positive electrode
secondary battery
ion secondary
sieve
recovered
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PCT/JP2012/062981
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English (en)
Japanese (ja)
Inventor
俊介 葛原
善弘 本間
藤田　浩示
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Ｄｏｗａエコシステム株式会社
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Publication of WO2012161168A1 publication Critical patent/WO2012161168A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • the present invention easily recycles valuable materials such as cobalt and nickel from the defective lithium ion secondary battery generated during the manufacturing process, and the positive electrode of the lithium ion secondary battery that is discarded with the life of the device and battery used.
  • the present invention relates to a method for recovering valuable materials from the positive electrode of a lithium ion secondary battery that can be recovered in a usable state.
  • Lithium ion secondary batteries are lighter, higher capacity, and higher electromotive force secondary batteries than conventional lead-acid batteries and nickel-cadmium secondary batteries, and are widely used in mobile devices such as mobile phones and laptop computers.
  • As a positive electrode material for such a lithium ion secondary battery lithium cobaltate (LiCoO 2 ), lithium nickelate (LiNiO 2 ), nickel-manganese-cobalt-based oxides, and the like are used. Cobalt and nickel are included. Therefore, it is desired to recover these valuable materials from the used lithium ion secondary battery and to recycle them as a positive electrode material for the lithium ion secondary battery.
  • the secondary metal foil coating waste material of the secondary battery in which the electrode material containing the metal compound is applied to the metal foil is heated to a temperature of 300 ° C. to 600 ° C. in a gas stream containing oxygen, and then subjected to a combustion treatment.
  • a combustion treatment method for metal foil coating waste materials of batteries has been proposed (see Patent Document 1).
  • the recovered material containing cobalt and nickel contains a large amount of aluminum as a current collector. Therefore, the recovered material cannot be used as it is as a reuse material of cobalt and nickel. For this reason, in order to use the recovered material as a reused raw material, more processes are required, and there is a problem that the recovery process becomes complicated.
  • the present invention relates to a valuable material from a positive electrode of a lithium ion secondary battery that can easily and efficiently recover a reused raw material containing valuable materials such as cobalt and nickel from the positive electrode of the lithium ion secondary battery.
  • the purpose is to provide a collection method.
  • Means for solving the problems are as follows. That is, ⁇ 1> a heating step of heating a positive electrode of a lithium ion secondary battery containing a current collector and a valuable material at 500 ° C. to 650 ° C .; And sieving the positive electrode after the heating step to obtain a recovered product containing the valuables and having a current collector content of 2% by mass or less. This is a method for recovering valuable materials from the positive electrode of the secondary battery.
  • ⁇ 3> The method for recovering a valuable material from the positive electrode of the lithium ion secondary battery according to any one of ⁇ 1> to ⁇ 2>, wherein the current collector is aluminum.
  • ⁇ 4> The method for recovering a valuable material from the positive electrode of the lithium ion secondary battery according to any one of ⁇ 1> to ⁇ 3>, wherein the valuable material is at least one of cobalt and nickel.
  • ⁇ 5> The lithium ion ion according to any one of ⁇ 1> to ⁇ 4>, wherein the sieve selection step uses a sieve having a mesh opening of 2.0 mm or less to obtain a recovered material under the sieve. This is a method for recovering valuable materials from the positive electrode of the secondary battery.
  • lithium that can solve the above-described problems and can easily and efficiently recover a reused raw material containing valuables such as cobalt and nickel from the positive electrode of a lithium ion secondary battery.
  • a method for recovering valuable materials from the positive electrode of an ion secondary battery can be provided.
  • FIG. 1 is a graph showing the relationship between the recovered particle size and the aluminum concentration and the relationship between the recovered particle size and the mass integrated value in Example 1.
  • FIG. 2 is a graph showing the relationship between the particle size of the recovered material and the aluminum concentration and the relationship between the particle size of the recovered material and the mass integrated value in Example 2.
  • FIG. 3 is a graph showing the relationship between the recovered particle size and the aluminum concentration and the relationship between the recovered particle size and the mass integrated value in Example 3.
  • FIG. 4 is a graph showing the relationship between the particle size of the recovered material and the aluminum concentration and the relationship between the particle size of the recovered material and the mass integrated value in Example 4.
  • FIG. 5 is a graph showing the relationship between the particle size of the recovered material and the aluminum concentration and the relationship between the particle size of the recovered material and the mass integrated value in Example 5.
  • FIG. 6 is a graph showing the relationship between the particle size of the recovered material and the aluminum concentration and the relationship between the particle size of the recovered material and the mass integrated value in Example 6.
  • FIG. 7 is a graph showing the relationship between the particle size of the recovered material and the aluminum concentration and the relationship between the particle size of the recovered material and the mass integrated value in Comparative Example 1.
  • FIG. 8 is a graph showing the relationship between the particle size of the recovered material and the aluminum concentration and the relationship between the particle size of the recovered material and the mass integrated value in Comparative Example 2.
  • FIG. 10A is a SEM photograph of the recovered material of Example 4.
  • FIG. 10B is a cobalt (Co) mapping image of the recovered product of Example 4.
  • FIG. 10C is a nickel (Ni) mapping image of the recovered material of Example 4.
  • the method for recovering valuable materials from the positive electrode of the lithium ion secondary battery of the present invention includes at least a heating step and a sieve sorting step, and further includes other steps as necessary.
  • the heating step is not particularly limited as long as the positive electrode of the lithium ion secondary battery is heated at 500 ° C. to 650 ° C., and can be appropriately selected according to the purpose.
  • the lithium ion secondary battery is not particularly limited and may be appropriately selected depending on the purpose.
  • a defective lithium ion secondary battery generated in the process of manufacturing a lithium ion secondary battery, used equipment examples thereof include a lithium ion secondary battery that is discarded due to a defect, a life of a device used, a used lithium ion secondary battery that is discarded due to a life.
  • the structure of the lithium ion secondary battery is not particularly limited as long as it has a positive electrode structure, and can be appropriately selected according to the purpose.
  • the positive electrode, the negative electrode, the separator, the electrolyte, and the organic solvent And a battery case made of metal containing the positive electrode, the negative electrode, the separator, and the electrolytic solution.
  • the shape of the lithium ion secondary battery is not particularly limited and may be appropriately selected depending on the intended purpose. Examples thereof include a cylindrical shape, a button shape, a coin shape, a square shape, and a flat shape.
  • Positive electrode- The positive electrode is not particularly limited as long as it is a positive electrode containing a current collector and a valuable material, and can be appropriately selected according to the purpose.
  • the current collector is applied to the current collector.
  • limiting in particular as a shape of the said positive electrode According to the objective, it can select suitably, For example, flat form etc. are mentioned.
  • the positive electrode material is not particularly limited as long as it contains the valuable material, and can be appropriately selected according to the purpose.
  • the positive electrode material includes at least a positive electrode active material containing the valuable material, and if necessary, a conductive agent. And a positive electrode material containing a binder resin.
  • the positive electrode active material include lithium cobalt oxide (LiCoO 2 ), lithium cobalt nickel oxide (LiCo 1/2 Ni 1/2 O 2 ), and LiNi x Co y Mn z O 2 (x + y + z) .
  • the electrically conductive agent there is no restriction
  • the binder resin is not particularly limited and may be appropriately selected depending on the intended purpose. For example, a homopolymer or copolymer such as vinylidene fluoride, tetrafluoroethylene, acrylonitrile, ethylene oxide, styrene-butadiene, etc. For example, rubber.
  • the heating step is performed on the positive electrode taken out from the battery case of the lithium ion secondary battery.
  • the method for taking out the positive electrode from the battery case is not particularly limited and may be appropriately selected depending on the purpose.
  • the battery case battery housing
  • the battery case is disassembled using a tool such as a pliers or a cutter.
  • a method of taking out the positive electrode in the battery case is not particularly limited and may be appropriately selected depending on the purpose.
  • the heating temperature is 500 ° C. to 650 ° C., preferably 590 ° C. to 610 ° C.
  • the heating temperature is less than 500 ° C.
  • the binder resin and the like contained in the positive electrode are not sufficiently decomposed, so that it is difficult to separate the current collector from the valuable material in the sieve sorting step.
  • the heating temperature exceeds 650 ° C., the current collector such as aluminum is oxidized and becomes brittle, so that it is difficult to separate the current collector from the valuable material in the sieve sorting step.
  • the current collector becomes brittle and thin, it is difficult to separate the current collector and the valuable material in the sieve selection step because the current collector and the valuable material are recovered together under the sieve. become.
  • the heating temperature is within the preferable range, it is advantageous in that the yield of recovered material that can be used as a reused raw material is high while suppressing energy used for heating.
  • the heating temperature refers to the temperature of the gas around the positive electrode during heating, for example, the temperature of the gas in the vicinity where the positive electrode is disposed in the heating furnace during heating.
  • the heating time is not particularly limited and may be appropriately selected depending on the intended purpose. It is preferably 0.5 hours to 6 hours, and more preferably 0.5 hours to 1 hour.
  • the heating is preferably performed using a furnace.
  • a furnace There is no restriction
  • a commonly used furnace such as a rotary kiln furnace can be used, and the selection range of the furnace is widened.
  • the binder resin in the positive electrode is usually an organic substance, it is thermally decomposed by the heating and hardly contained in the recovered material.
  • the recovered material containing the valuable material can be used as a reuse material.
  • a step of removing the current collector from the recovered material when the recovered material is reused for example, a step of sorting aluminum, etc. It becomes necessary and the process at the time of reuse becomes complicated.
  • the recovered product under a sieve having a sieve mesh opening of 2.0 mm or less, and obtaining the recovered product under a sieve having a sieve mesh opening of 1.2 mm or less. More preferably, it is particularly preferable to obtain the recovered material under a sieve having a sieve mesh opening of 0.6 mm or less. If the mesh opening exceeds 2.0 mm, the content of the current collector in the recovered product may increase.
  • the sieving may be dry or wet.
  • the pulverization step is not particularly limited as long as it is a step before the sieve selection step and after the heating step without pulverizing the current collector and pulverizing the positive electrode. You can choose.
  • the pulverization step in the sieving selection step, the separation efficiency of the current collector and the valuable material is improved, and the yield of the recovered product obtained is increased.
  • the current collector such as aluminum is not stretched and pulverized.
  • the positive electrode material containing the valuable material is easily pulverized by the heating step.
  • a hammer crusher, a rod mill, a ball mill, a jaw crusher, a roll crusher, a cutter mill, or a rotary crusher can be used.
  • the concentration step is not particularly limited as long as it is a step of concentrating the valuables in the recovered product after the sieve sorting step, and can be appropriately selected according to the purpose.
  • the recovered product And a step of mixing and baking, and washing with water.
  • the firing temperature is not particularly limited and may be appropriately selected depending on the intended purpose, but is preferably 650 ° C. to 800 ° C.
  • Example 1 ⁇ Recovery of valuable materials> A used lithium ion secondary battery for a personal computer was used. The used lithium-ion secondary battery for personal computers was disassembled with a tool, and the positive electrode was taken out from the battery case. A total amount of 1,000 g of the extracted positive electrode contained 100 g of an aluminum foil as a current collector and 900 g of a positive electrode material containing a valuable material.
  • the heated positive electrode is a multi-stage sieve (7 stages) in which sieves of 0.075 mm, 0.15 mm, 0.3 mm, 0.6 mm, 1.2 mm, 2.0 mm, and 10 mm are stacked in this order. And screened.
  • the aluminum concentration (Al concentration) was determined for each sieve and the recovered material after sieving. Moreover, the mass integration value from the finer particle size was calculated
  • the particle size was “over 0.075 mm and not more than 0.15 mm” (in the figure, It is expressed as “0.15 / 0.075”).
  • the ratio (mass ratio) of the recovered material having a current collector content of 2% by mass or less to the total recovered material is shown in Table 1 and FIG.
  • Example 2-6 and Comparative Examples 1-2 valuable materials were collected in the same manner as in Example 1 except that the heating temperature was changed to the heating temperature shown in Table 1.
  • the aluminum concentration (Al concentration) was determined for each sieve and the recovered material after sieving.
  • the mass integration value from the finer particle size was calculated
  • the ratio (mass ratio) of the recovered material having a current collector content of 2% by mass or less to the total recovered material is shown in Table 1 and FIG.
  • Examples 1 to 6 from the results shown in FIGS. 1 to 6 and 9 and Table 1, a collected material having a current collector content of 2% by mass or less, that is, a recycled material can be collected, and a collected material after sieve screening.
  • the mass ratio in was about 40% by mass or more, and the recycled material could be recovered with high efficiency.
  • the heating temperature was 590 ° C. to 610 ° C.
  • a recovered material with a higher efficiency and a current collector content of 2 mass% or less could be recovered.
  • FIGS. 10A to 10C The analysis results of the recovered material (particle size of 0.075 mm or less) remaining under the sieve having a sieve mesh of 0.075 mm in Example 4 are shown in FIGS. 10A to 10C.
  • FIG. 10A is a SEM photograph of the recovered material.
  • FIG. 10B is a cobalt (Co) mapping image of the recovered material.
  • FIG. 10C is a nickel (Ni) mapping image of the recovered material. From these results, it was confirmed that the recovered material contains cobalt and nickel which are valuable materials.
  • the method for recovering valuable materials from the positive electrode of the lithium ion secondary battery according to the present invention is capable of easily and efficiently recovering reused raw materials containing valuable materials such as cobalt and nickel from the positive electrode of the lithium ion secondary battery. Therefore, the method can be suitably applied to a method for recovering valuable materials from a used lithium ion secondary battery.

Abstract

L'invention concerne un procédé de récupération de matériaux de valeur dans l'électrode positive d'un accumulateur lithium-ion qui comprend un collecteur contenant de l'aluminium et un matériau de valeur comprenant au moins soit du cobalt, soit du nickel, le procédé comprenant : une étape de chauffage dans laquelle l'électrode positive de l'accumulateur lithium-ion est chauffée à une température de 500 à 600 °C, de préférence de 590 à 610 °C ; et une étape de tamisage dans laquelle l'électrode positive, après l'étape de chauffage, est tamisée avec un tamis ayant une ouverture de maille inférieure ou égale à 2,0 mm et le matériau récupéré contenant le matériau de valeur et comprenant une partie du collecteur inférieure à 2 % en masse.
PCT/JP2012/062981 2011-05-25 2012-05-22 Procédé de récupération de matériaux de valeur dans l'électrode positive d'un accumulateur lithium-ion WO2012161168A1 (fr)

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JP2011117229A JP6100991B2 (ja) 2011-05-25 2011-05-25 リチウムイオン二次電池の正極からの有価物の回収方法
JP2011-117229 2011-05-25

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN114068909A (zh) * 2021-11-10 2022-02-18 中南大学 一种退役ncm正极料再生ncma正极材料的方法

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JP6483569B2 (ja) * 2015-08-13 2019-03-13 Ｊｘ金属株式会社 リチウムイオン電池の処理方法
KR102249266B1 (ko) * 2018-11-13 2021-05-06 부경대학교 산학협력단 니켈 및 코발트 회수 방법
KR20220001363A (ko) 2020-06-29 2022-01-05 주식회사 엘지에너지솔루션 양극 스크랩을 이용한 활물질 재사용 방법

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JPH108150A (ja) * 1996-06-21 1998-01-13 Tama Kagaku Kogyo Kk 二次電池の金属箔塗着廃材の燃焼処理法
JP2003272720A (ja) * 2002-03-15 2003-09-26 Japan Science & Technology Corp コバルト酸リチウムの回収方法
JP2010231925A (ja) * 2009-03-26 2010-10-14 Nippon Denko Kk マンガン系リチウムイオン二次電池の有価資源回収方法その装置
JP2011094228A (ja) * 2009-09-30 2011-05-12 Dowa Eco-System Co Ltd リチウムの回収方法
JP2012079630A (ja) * 2010-10-05 2012-04-19 Dowa Eco-System Co Ltd リチウムイオン二次電池からの有価物の回収方法、及び有価物を含有する回収物

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JPH108150A (ja) * 1996-06-21 1998-01-13 Tama Kagaku Kogyo Kk 二次電池の金属箔塗着廃材の燃焼処理法
JP2003272720A (ja) * 2002-03-15 2003-09-26 Japan Science & Technology Corp コバルト酸リチウムの回収方法
JP2010231925A (ja) * 2009-03-26 2010-10-14 Nippon Denko Kk マンガン系リチウムイオン二次電池の有価資源回収方法その装置
JP2011094228A (ja) * 2009-09-30 2011-05-12 Dowa Eco-System Co Ltd リチウムの回収方法
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Publication number Priority date Publication date Assignee Title
CN114068909A (zh) * 2021-11-10 2022-02-18 中南大学 一种退役ncm正极料再生ncma正极材料的方法

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